Classifications

• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M10/00—Secondary cells; Manufacture thereof
  • H01M10/05—Accumulators with non-aqueous electrolyte
  • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
  • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
  • H01M10/0562—Solid materials
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
  • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
  • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
  • H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
  • H01B1/122—Ionic conductors
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M10/00—Secondary cells; Manufacture thereof
  • H01M10/05—Accumulators with non-aqueous electrolyte
  • H01M10/052—Li-accumulators
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M6/00—Primary cells; Manufacture thereof
  • H01M6/14—Cells with non-aqueous electrolyte
  • H01M6/18—Cells with non-aqueous electrolyte with solid electrolyte
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M10/00—Secondary cells; Manufacture thereof
  • H01M10/05—Accumulators with non-aqueous electrolyte
  • H01M10/052—Li-accumulators
  • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M10/00—Secondary cells; Manufacture thereof
  • H01M10/05—Accumulators with non-aqueous electrolyte
  • H01M10/058—Construction or manufacture
  • H01M10/0585—Construction or manufacture of accumulators having only flat construction elements, i.e. flat positive electrodes, flat negative electrodes and flat separators
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M2300/00—Electrolytes
  • H01M2300/0017—Non-aqueous electrolytes
  • H01M2300/0065—Solid electrolytes
  • H01M2300/0068—Solid electrolytes inorganic
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
  • Y02E60/10—Energy storage using batteries
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
  • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
  • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

• the present invention relates to an all solid state battery, and more particularly to a solid electrolyte used in an all solid state thin film lithium secondary battery.
• an electrolyte composed of a liquid such as an organic solvent is used as a medium for moving ions. This may cause problems such as electrolyte leakage from the battery.
• lithium halide lithium nitride, lithium oxyacid salt, derivatives of these, etc.
• lithium nitride phosphate obtained by introducing nitrogen N into lithium orthophosphate (Li 3 P 0 4 )
• the phosphorus atoms (P) constituting the lithium nitride phosphate react with water molecules in the wet atmosphere. At this time, the phosphorus atom is reduced from the +5 oxidation state to a lower oxidation state. As a result, lithium nitride phosphate is decomposed and its ion conductivity is significantly reduced.
• An object of the present invention is to provide a solid electrolyte capable of suppressing the decrease in ion conductivity even in a wet atmosphere, and an all-solid battery using such a solid electrolyte. Disclosure of the invention
• the solid electrolyte of the present invention has the general formula:
• y 1. 0 5 0 to 3. 9
• z 0. 0 1 to 0. 5 0).
• x 0.6 to 1.
• y 1.05 to 1. 9 8 5.
• z 0. 0 1 to 0. 50.
• x l. 6 to 2.
• y 3. 0 to 3. 98 5.
• z 0. 0 1 to 0. 50.
• x 2.6 to 3.0
• y 2.0 to 50 to 2.98 5.
• z 0.0 to 1 to 50 are more preferable.
• the present invention also relates to an all-solid battery comprising a positive electrode, a negative electrode, and the above-mentioned solid electrolyte disposed between the positive electrode and the negative electrode.
• FIG. 1 is a schematic longitudinal sectional view of a test cell for solid electrolyte evaluation in an example of the present invention.
• FIG. 2 is a schematic vertical sectional view of the all-solid-state battery in the example of the present invention.
• the solid electrolyte of the present invention can be prepared by using Li (lithium), O (oxygen), N (nitrogen), Si (Ge), B (boron), Ge (germanium), A 1 (aluminum), C (carbon) And at least one element M selected from the group consisting of Ga (gallium) and S (sulfur).
• this solid electrolyte consists of a nitride of lithium oxyacid salt containing the element M.
• lithium oxo-nitride is lithium oxo-oxide of oxygen A part is nitrogenated.
• x, y and z indicate atomic ratios of L L, O. and N to the element M, respectively.
• lithium nitride phosphoric acid which is a solid electrolyte conventionally used, easily reacts with moisture when it is left in a wet atmosphere, and its ion conductivity significantly decreases. This is due to the fact that some P (phosphorus) contained in lithium nitride phosphate reacts with the moisture in the atmosphere and is reduced from +5 valence.
• the solid electrolyte according to the present invention has an element M which forms a more stable bond with oxygen thermodynamically as compared with the bonded state of phosphorus and oxygen in lithium lithium phosphate.
• the structure of the solid electrolyte can be stabilized, and the decrease in ion conductivity of the solid electrolyte in a wet atmosphere can be suppressed.
• z in the above general formula is from 0.10 to 0.50, high ion conductivity can be obtained, and the decrease in ion conductivity due to storage in a wet atmosphere can be suppressed. If z is less than 0.1, it will be difficult to maintain high ion conductivity. In addition, when z exceeds 0.50, the ionic conductivity tends to decrease due to the breakage of the solid electrolyte framework structure. When such a solid electrolyte with reduced ion conductivity is used for the all solid battery, the resistance of the solid electrolyte is increased, and the charge and discharge characteristics are significantly reduced. Furthermore, it is more preferable that z is 0.;! To 0.5. The structural distortion of the solid electrolyte increases the lithium ion conduction channel.
• composition of the solid electrolyte changes depending on the type of element M used. That is, X and y in the above general formula depend on the composition and type of lithium oxyacid salt used as the raw material. For this reason, X is in the range of 0.6 to 5.0, and y is in the range of 1.005 to 3.925.
• the above-mentioned solid electrolyte may contain elements other than those described above as long as the effects of the present invention are not impaired.
• the solid electrolyte of the present invention can be obtained, for example, by substituting a part of the oxygen atom of lithium oxyacid salt with a nitrogen atom.
• lithium oxy acid salt is L i B i ⁇ 2 , L i A 1 2 2 or L i G a ⁇ 2 , ie, in the above general formula, M is B i, A 1 or G a , X is from 0.6 to 1: 1.0, y is from 1. 0 5 0 to: I. 9 85, and z is from 0. 0 to 0. 50.
• lithium oxy acid salt is L i 2 S i O 3 , L i 2 G e O 3 or L i 2 C O 3, that is, in the above general formula, M is S i, G e or C , X is preferably 1. 6 to 2. 0, y is preferably 2. 0 50 to 2. 9 85, and z is preferably 0. 0 1 to 0.50.
• lithium oxy acid salt is Li 2 S 4 4, that is, in the above general formula, when M is S, X is 1. 6 to 2. 0 and y is 3. 0 5 to 3 9 85 and z are preferably in the range of 0. 0 1 to 0. 50.
• lithium oxy acid salt is L i 3 B i 0 3
• X is 2. 6 to 3.
• y is 2. 0 5 0 to 2.
• 9 85 and z are preferably in the range of 0. 0 1 to 0. 50.
• the lithium oxy acid salt is L i 4 S i 0 4 or L i 4 G e 0 4 , that is, in the above general formula, when M is S i or G e, X is 3. 6 to 6 It is preferred that 4.0, y be from 3.005 to 3.985, and that z be from 0. 0 to 0.50. If the lithium oxyacid salt is L IS A 1 ⁇ 4, i.e. in the above general formula, when M is A 1, X is 4.. 6 to 5. 0, y 3. 0 5 0-3. It is preferable that 9 85 and z be 0.01 to 0.50.
• the solid electrolyte according to the present invention is preferably in the form of a thin film. The film thickness can be suitably controlled, but is preferably 0.1 to 10.
• the solid electrolyte according to the present invention may be either crystalline or amorphous.
• Examples of the method for producing a solid electrolyte of the present invention include a method for producing a thin film formation technique using a vacuum apparatus, as in the case of producing lithium nitride phosphate which is a conventional solid electrolyte. Of course, other methods may be used.
• a method for producing a thin film for example, a sputtering method in which a target is sputtered with nitrogen (N 2 ) by means such as a magnetron or a high frequency, or a method combining evaporation and ion beam irradiation introducing nitrogen ions.
• N 2 nitrogen
• a resistance heating vapor deposition method in which a vapor deposition source is heated by vapor deposition by resistance
• an electron beam vapor deposition method in which a vapor deposition source is heated by vapor deposition by an electron beam
• a vapor deposition source by vapor deposition by laser A laser ablation method etc.
• the above-mentioned lithium oxyacid salt is used as a vacuum or evaporation source.
• the resulting mixture may be used as a target or a deposition source.
• the target or vapor deposition source in addition to the lithium oxyacid salt of an L i 2 ⁇ , a mixture of lithium oxyacid salt, or a L i 2 0, S i ⁇ 2, B i 2 ⁇ 3, G E_ ⁇ 2, a l 2 ⁇ 3, or may be a mixture of G a 2 O 3.
• the all-solid-state battery according to the present invention can be obtained by using the above-mentioned solid electrolyte.
• FIG. 2 shows a schematic longitudinal sectional view of the all-solid thin-film lithium secondary battery.
• the all solid thin film lithium secondary battery includes a substrate 21 and a first current collector 22 provided on the substrate 21, a first electrode 23, a solid electrolyte 24 according to the present invention, and a second electrode 2. 5 and the second current collector 26
• the first electrode is a positive electrode layer and the second electrode is a negative electrode layer
• the first electrode may be a negative electrode layer and the second electrode may be a positive electrode layer.
• This battery is manufactured by a thin film production method using a vacuum device, from the top of the substrate 21 to the first current collector 22, the first electrode 23, the solid electrolyte 24, the second electrode 25, the second current collector 2 It is obtained by laminating in the order of 6.
• any method other than the thin film manufacturing method using a vacuum device may be used.
• a resin or an aluminum laminate film is disposed on the second current collector 26 as a protective layer.
• an electrically insulating substrate such as alumina, glass, and polyimide film, a semiconductor substrate such as silicon, or a conductive substrate such as aluminum and copper can be used.
• a conductive substrate the interface between the first current collector 22 and the substrate 21 or the interface between the first current collector 22 and the substrate 21 so that the first current collector 22 and the second current collector 26 do not conduct.
• a material having an electrical insulating property is provided on at least one of the interfaces between the second current collector 26 and the substrate 21. Deploy.
• the surface roughness of the substrate surface is preferably small, it is effective to use a mirror plate or the like.
• the first current collector 22 disposed on the substrate 21 is, for example, platinum, platinum / palladium, gold, silver, aluminum, copper, an electron conducting material such as ITO (indium monostannic oxide film), etc. Materials are used. Other than these materials, any material that has electron conductivity and does not react with the first electrode 23 can be used as a current collector.
• the first current collector 22 As a method of producing the first current collector 22, a sputtering method, a resistance thermal evaporation method, an ion beam evaporation method, an electron beam evaporation method, or the like is used. However, when a conductive material such as aluminum, copper or stainless steel is used for the substrate 21, the first current collector 22 may not be disposed.
• the first electrode (positive electrode layer) 2 for example, lithium cobalt oxide used as a cathode material for lithium secondary battery (L i C o O, nickel acid lithium ⁇ beam (L i N i ⁇ 2), and manganese lithium acid (L i Mn 2 Rei_4), rabbi vanadium oxide (V 2 ⁇ 5), molybdenum oxide (Mo 0 3), be used transition metal oxide such as sulfide titanium (T i S 2)
• any material used for the positive electrode of a lithium secondary battery can be used for the first electrode 23.
• a sputtering method As a method of producing the first electrode (positive electrode layer) 23, a sputtering method, a resistance heating evaporation method, an ion beam evaporation method, an electron beam evaporation method, a laser ablation method, or the like is used.
• the above-mentioned solid electrolyte according to the present invention is used.
• the second electrode (negative electrode layer) 25 includes, for example, a graphite material used as a negative electrode material of a lithium secondary battery and a carbon material (C) such as hard carbon, and an alloy containing tin (Sn), lithium cobalt Nitride It is preferable to use (LiCoN), lithium metal (Li), and lithium alloy (e.g. Lia1). Other than these materials, any material used for the negative electrode of a lithium secondary battery can be used for the second electrode 25.
• a sputtering method As a method of manufacturing the second electrode (negative electrode layer) 25, a sputtering method, a resistance heating evaporation method, an ion beam evaporation method, an electron beam evaporation method, a laser ablation method, or the like is used.
• the same material as that of the first current collector 22 is used as the second current collector 26 (as a method of producing the second current collector 26, it is the same as that of the first current collector 22 The following method is used.
• an all solid thin film lithium secondary battery is shown as an example of the all solid battery according to the present invention, but the present invention is not limited to only this battery.
• test cell for evaluating a solid electrolyte was produced in the procedure shown below.
• a schematic longitudinal sectional view of the test cell is shown in FIG.
• a metal mask having a window of 20 mm ⁇ 10 mm in size is placed at a predetermined position on the mirror-surfaced silicon substrate 11 whose surface roughness is less than 30 nm is oxidized.
• a film made of platinum was formed by the rf magnetron sputtering method to obtain a platinum current collector layer 12 having a film thickness of 0.5 ( as a second step, the platinum current collector obtained above).
• Body layer 12 on A metal mask having a window with a size of 15 mm ⁇ 15 mm was placed, and a solid electrolyte thin film made of a nitride of lithium oxyacid salt shown in Table 1 was formed by rf magnetron sputtering method. m solid electrolyte layer 13 was obtained.
• lithium oxo-oxide shown in Table 1 was used as a target, and nitrogen (N 2 ) was used as sputtering gas.
• N 2 nitrogen
• the internal pressure of the chamber was 2. 7 Pa
• the gas introduction amount was 10 sccm
• the sputtering time was 2 hours.
• the high frequency power applied to the target was 200 W.
• a metal mask having a window of 10 mm ⁇ 10 mm in size is disposed on the solid electrolyte layer 13 obtained above so as not to protrude from the solid electrolyte layer 13.
• a film made of platinum was formed by an rf magnetron sputtering method to obtain a platinum current collector layer 14 with a film thickness of 0.5. Comparative example 1
• lithium nitride phosphate is prepared in the same manner as in Example 1.
• each of the test cells of Examples 1 to 10 and Comparative Example 1 prepared above was tested in a thermostatic chamber with a humidity of 50% and a temperature of 20 ° C. I saved it for 2 weeks. Then, for each test cell, perform AC impedance measurement immediately after production and after storage for 2 weeks. The change in ion conductivity with time was examined. At this time, as a condition of the AC impedance measurement, the equilibrium voltage is zero, ⁇ 1 0 m V, the frequency domain amplitude of the applied voltage was 1 0 5 ⁇ 0. 1 H z. The ion conductivity was determined from the measurement results.
• the evaluation results are shown in Table 1.
• the ionic conductivity was expressed as an index relative to the ionic conductivity obtained as a result of the measurement of the impedance immediately after the test cell preparation as 100.
• Table 1 The ionic conductivity was expressed as an index relative to the ionic conductivity obtained as a result of the measurement of the impedance immediately after the test cell preparation as 100.
• Example 1 Li 4 Si 04, L 1 BO 2 Ll 2.3 D 10.5 ⁇ ⁇ . 5 ⁇ 2. 45 ⁇ ⁇ . 3 10 0.00 85. 08
• Example 1 2 Li 4 Si 04, L GeOs Li 3.8 Sl 0.5 Geo. 503. 45 No .3 100.00 90.05 example 1 3 L14S1O4, L12CO3 Li 2.8S10.5 C0.5O2.95N0.3 100.00 83.62
• Example 1 6 LiB 0 2 1 L 15 AIO 4 Li 2.8 B 0.5 AI 0.5 O 2. 45 N 0.3 10 0.00 83.
• Example 1 7 Li B 0 2 , L12 CO3 Li 1.3 B 0.5 C 0.5 O 1. 95 J 0.3 10 0.00 78.70
• Example 1 8 LiB 02, Li Ga 0 2 Li. . ⁇ . ⁇ Gao. 50 i. 45 No. 3 100.00 81.33
• Example 2 0 Li 4 Ge 04, L 12 CO 3 Li 2.8 Geo. 5 C 0.5 O 2. 95 N 0.3 10 0.00 83.
• Example 2 1 Li 4 Ge 04, L 12 SO 4 Li 2.8 Geo. 5 So. 503 No. 3 100.00 83.20 example 2 2 LiGa0 2, L15AIO4 Li 2.8Gao.5 AI0.5O2.45N0.3 100.00 85.03 example 2 3 L12SO4, Li 2 C0 3 Li 1.8S0.5 C0.5O2.95N0.3 100.00 76.77 From Table 2, in Examples 1 to 2, it was found that the decrease in ion conductivity was suppressed after storage in a wet atmosphere, and the deterioration of the solid electrolyte was suppressed.
• the molar ratio of nitrides of two types of lithium oxyacid salts is 1: 1, but other molar ratios may be used. Examples 2 to 4 and Comparative Examples 2 to 4
• Lithium orthosilicate as target in the second step Lithium orthosilicate as target in the second step
• Example A solid electrolyte layer shown in Table 3 was obtained by the same method as in 1.
• a test cell was produced in the same manner as in Example 1 except for this second step.
• Example 26 The test cell was evaluated by the method similar to Example 1. The evaluation results are shown in Table 3.
• the ion conductivity immediately after the preparation of the test cell is shown as an index to the ion conductivity when the atomic ratio of nitrogen to carbon is 0.3 (Example 26) as 100.
• Table 3 The ion conductivity was expressed as an index relative to the ion conductivity immediately after preparation of the test cell as 100.
• the ion conductivity immediately after the preparation of the test cell is shown as an index to the ion conductivity when the atomic ratio of nitrogen to carbon is 0.3 (Example 26) as 100.
• the all-solid-state battery having the configuration shown in FIG. 2 was produced by the following procedure.
• a metal mask having a window of 20 mm ⁇ 12 mm in size is disposed at a predetermined position on the mirror-surfaced silicon substrate 11 whose surface roughness is not more than 30 nm and is oxidized.
• a film made of platinum was formed by the rf magnetron sputtering method to obtain a first current collector 22 with a film thickness of 0.5 m.
• a metal mask having a window of 10 mm ⁇ 10 mm in size is disposed on the first current collector 22 obtained above, and the rf magnetron sputtering method is used.
• a thin film of lithium cobaltate (L i C o 0 2 ) was formed to obtain a first electrode (positive electrode layer) 23 with a film thickness of 1. O ⁇ m.
• a metal mask having a window of 15 mm ⁇ 15 mm in size is disposed on the first electrode 23 obtained above, and the results are shown in Table 4 by the rf magnetotron sputtering method.
• a thin film composed of a lithium oxyacid salt nitride was formed to obtain a solid electrolyte 24 with a thickness of 1.0 tm.
• lithium oxo-oxide shown in Table 4 was used as the target, and nitrogen (N 2 ) was used as the sputtering gas.
• nitrogen (N 2 ) was used as the sputtering gas.
• the internal pressure of the tamper is 2.7 Pa
• the amount of gas introduced is 10 sccm
• the sputtering time is 2 hours.
• the high frequency power applied to the target was 200 W.
• a metal mask having a window of lO mm x 1 O mm is placed on the solid electrolyte 24 obtained above, and a thin film made of lithium metal is formed by resistance heating evaporation, The second electrode (negative electrode layer) 25 with a thickness of 0.5 im was obtained.
• a metal mask having a window of 20 mm ⁇ 12 mm in size is disposed on the second electrode 25 obtained above, and the metal mask is not in contact with the first current collector 22.
• a thin film made of copper was formed by an rf magnetron sputtering method so as to completely cover the negative electrode layer 25 to obtain a second current collector 26 with a film thickness of 1. O ⁇ m. Comparative example 5
• lithium orthophosphate is used as a target, and lithium nitride phosphate is prepared in the same manner as in Example 3 1
• a thin film of (Li 2. 8 P 0 3. 45 No. 3 ) was formed to obtain a solid electrolyte having a thickness of 1.0 m.
• a battery was produced in the same manner as in Example 30 except for this third step.
• each of the all-solid-state batteries of Examples 2 to 7 and Comparative Example 5 prepared above was subjected to a thermostatic chamber with a relative humidity of 50% and a temperature of 20 ° C. I saved it for 2 weeks. Then, for each battery, AC impedance measurements were performed immediately after preparation and after storage for 2 weeks. At this time, as a condition of the AC impedance measurement, the equilibrium voltage is zero, the amplitude of the voltage to be marked pressure is 1 0 mV, the frequency domain is set to 1 0 5 ⁇ 0. 1 H z . The internal impedance was determined from the measurement results.
• Table 4 shows the measurement results of internal impedance.
• the internal impedance is shown as an index relative to the internal impedance immediately after battery fabrication as 100.

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